Organic waste acid water treatment device

Abstract

According to the organic waste acid water treatment device, organic matter in organic waste acid water is extracted and subjected to liquid separation through the extraction kettle, meanwhile, the distillation kettle is arranged to distill an extracted water phase, and an acid-water mixture in the water phase is distilled and recycled; after kettle residues in the distillation kettle are cooled and separated out, solid waste and centrifugal mother liquor are separated out in a centrifugal mode, and the centrifugal mother liquor is recycled by the distillation kettle. According to the device, the organic waste acid water generated in heliotropin synthesis is classified and recycled through cooperative use of the equipment, the device has the advantages of saving resources and reducing pollution, and the defect that in an existing method for treating the waste acid water in heliotropin synthesis, recoverable substances cannot be fully recycled, so that resources are wasted is overcome.

Description

Technical Field

[0001] The present application relates to the technical field of wastewater treatment, and in particular to a device for treating organic waste acid water. Background Art

[0002] Piperonal is an important chemical raw material, widely used in the synthesis of cosmetics, medicines, pesticides and metal electroplating. The traditional preparation method of piperonal is to use safrole extracted from plants as raw materials, and then isomerize and oxidize it. This traditional preparation method is limited by the natural safrole resources, has a lengthy preparation process, high costs, and serious environmental pollution. It is not suitable for large-scale industrial production, and the product cannot meet market demand. The chemical synthesis of piperonal has more advantages than the preparation of natural raw materials, and has become a research hotspot.

[0003] The existing industrial synthesis method of piperonal is mainly the glyoxylic acid method, which is to prepare 3,4-methylenedioxyphenylglycolic acid from pepper, and then oxidize 3,4-methylenedioxyphenylglycolic acid with nitric acid to prepare piperonal. In this method, due to the use of nitric acid for oxidation, a large amount of organic waste acid water will be generated after the reaction. The existing method for treating the waste acid water is mainly to separate the oil phase after the waste acid water is statically layered, and then add alkali to the waste water of the aqueous phase, neutralize it, and then discharge it into the sewage treatment workshop for treatment. However, although this method can treat the waste acid water, a large amount of salt will be generated during the neutralization process. The neutralized waste water not only has high salt content, but also has high COD value, which will increase the load and production cost of the biochemical station, and the recyclable substances in the waste water cannot be fully recycled, resulting in a waste of resources. Utility Model Content

[0004] The present application provides an organic waste acid water treatment device, which is used to solve the problem of resource waste caused by failure to fully recycle recyclable materials in the existing method for treating waste acid water in piperonal synthesis.

[0005] The present application provides an organic waste acid water treatment device, comprising a wastewater storage tank, an extraction kettle, a liquid transfer pump, a distillation kettle, a centrifuge and a mother liquid storage tank connected in series in sequence;

[0006] The still is also connected in series with the dilute nitric acid storage tank and the reaction kettle;

[0007] The mother liquor storage tank is also connected to the distillation kettle;

[0008] The centrifuge is also connected to the solid waste storage tank;

[0009] The extraction kettle is also connected to the extractant storage tank, and the extraction kettle is also connected to the liquid transfer pump and the extraction liquid storage tank through valves respectively.

[0010] Optionally, the extraction kettle comprises an extraction kettle body and a filter;

[0011] The filter is arranged at the lower part of the extraction kettle body and is connected through a connecting pipe;

[0012] A valve is arranged on the connecting pipe.

[0013] Optionally, a stirring paddle is provided in the extraction kettle;

[0014] The outer side wall of the extraction kettle body is provided with a jacket.

[0015] Optionally, a balance pipe is also provided on the top of the extraction kettle body;

[0016] A filter box is connected to the balance pipe.

[0017] Optionally, multiple layers of filter screens are arranged in the filter along the liquid flow direction;

[0018] The mesh openings of the multi-layer filter gradually decrease along the direction of liquid flow;

[0019] The connection mode between the filter and the connecting pipe is a detachable connection.

[0020] Optionally, one end of the filter box is connected to the balance pipe, and the other end is closed by an end cover, and the side of the filter box is a hollow structure;

[0021] A porous partition is arranged at one end of the filter box close to the balance pipe, and granular activated carbon is filled between the porous partition and the end cover.

[0022] Optionally, the solid waste storage tank is connected to a solid waste treatment device;

[0023] The solid waste treatment device is an incinerator or a cracking furnace.

[0024] The present application provides an organic waste acid water treatment device, which extracts organic matter in the organic waste acid water by using an extractant by setting an extraction kettle, recovers it after liquid separation, and simultaneously sets a distillation kettle to distill the aqueous phase after extraction, recovers the acid-water mixture in the aqueous phase by distillation, and separates the solid waste and the centrifugal mother liquor by centrifugation after cooling and precipitation in the distillation kettle, and recovers the centrifugal mother liquor by recycling the centrifugal mother liquor and recycling it by using the distillation kettle again. The device of the present application, through the coordinated use of the above-mentioned equipment, classifies and recovers the organic waste acid water generated in the synthesis of piperonal, has the advantages of saving resources and reducing pollution, and overcomes the disadvantage of the existing method for treating waste acid water in the synthesis of piperonal, which fails to fully recycle the recyclable materials and causes waste of resources. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, a brief introduction will be given below to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0026] Figure 1 A schematic diagram of an organic waste acid water treatment device provided in one embodiment of the present application;

[0027] Figure 2 A schematic diagram of the structure of an extraction kettle provided in one embodiment of the present application;

[0028] Figure 3 A schematic diagram of the structure of a filter provided in one embodiment of the present application;

[0029] Figure 4 A schematic diagram of the structure of a filter box provided in one embodiment of the present application;

[0030] Figure 5 A schematic diagram of an organic waste acid water treatment device provided in another embodiment of the present application.

[0031] Description of reference numerals:

[0032] 1. Wastewater storage tank; 2. Extraction kettle; 3. Distillation kettle; 4. Centrifuge; 5. Mother liquor storage tank; 6. Dilute nitric acid storage tank; 7. Reactor; 8. Extraction liquid storage tank; 20. Extraction agent storage tank; 21. Extraction kettle body; 22. Filter; 23. Connecting pipe; 41. Solid waste storage tank; 42. Solid waste treatment device; 71. Liquid transfer pump; 100. Valve; 211. Agitator; 212. Balance pipe; 213. Filter box; 221. Filter screen; 2131. End cover; 2132. Porous partition. DETAILED DESCRIPTION

[0033] In order to make the purpose, technical scheme and advantages of the embodiments of the present application clearer, the technical scheme in the embodiments of the present application is clearly and completely described below. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work also fall within the scope of protection of the present application.

[0034] like Figure 1 As shown, the present application provides an organic waste acid water treatment device, comprising a wastewater storage tank 1, an extraction kettle 2, a liquid transfer pump 71, a distillation kettle 3, a centrifuge 4 and a mother liquid storage tank 5 connected in series in sequence;

[0035] The distillation kettle 3 is also connected in series with the dilute nitric acid storage tank 6 and the reaction kettle 7;

[0036] The mother liquid storage tank 5 is also connected to the still 3;

[0037] The centrifuge 4 is also connected to the solid waste storage tank 41;

[0038] The extraction kettle 2 is also connected to the extractant storage tank 20, and the extraction kettle 2 is also connected to the liquid transfer pump 71 and the extract storage tank 8 through valves.

[0039] When in use, the waste acid water temporarily stored in the wastewater storage tank 1 is transferred to the extraction kettle 2 to an appropriate liquid level, and then the extractant (ethylene dichloride in this application) in the extractant storage tank 20 is added to the extraction kettle 2 to an appropriate liquid level. The liquid in the extraction kettle 2 is stirred, and the organic compounds (such as piperonal, 3,4-methylenedioxyphenylethanolic acid, piperonyl ring and other organic substances) in the waste acid water are extracted by the extractant. After the extraction in the extraction kettle 2 is completed, the liquid is allowed to stand for 20 to 30 minutes to allow it to be completely stratified. Since the specific gravity of the extractant (ethylene dichloride, specific gravity of about 1.25) is greater than the specific gravity of water (the specific gravity of water is 1), the extractant is in the lower layer, that is, the oil phase, and the lower oil phase, that is, the extract, is released and transferred to the extract storage tank 8 for recovery.

[0040] The upper aqueous phase in the extraction kettle 2, i.e., the waste acid water, is pumped into the distillation kettle 3 through the liquid transfer pump 71, and the distillation kettle 3 is heated at this time (the heating method can be steam or an electric heater is arranged in the distillation kettle 3. In this application, steam heating is adopted, i.e., high-temperature and high-pressure steam is introduced into the jacket of the distillation kettle 3). In this application, for example, the temperature of the liquid in the kettle is heated to 120-140°C. At this time, the water in the waste acid water and the azeotrope of nitric acid-water will be evaporated, and the evaporated gaseous substance will be condensed into liquid in the condenser on the distillation kettle 3 (in the present application, the evaporated gaseous substance is condensed into liquid in the gaseous state and cooled to 30-50°C and then extracted from the condenser of the distillation kettle 3). The condensate extracted from the distillation kettle 3, that is, the dilute nitric acid (with a mass concentration of less than 5%) is transferred to the dilute nitric acid storage tank 6 to prepare the dilute nitric acid of the required concentration for the reaction (in the present application, the dilute nitric acid with a mass concentration of 10% is used for the reaction). The dilute nitric acid prepared in the dilute nitric acid storage tank 6 can be used for the reaction in the reactor 7.

[0041] After the acid water in the still 3 is distilled, some still residues that have not been distilled out still remain in the still. At this time, the heating of the still is stopped, and the still 3 is cooled by circulating water. Since the residues in the still are by-products generated during the reaction (such as substances polymerized between substrates), these substances in the still residue will precipitate as solids after cooling. After the substances in the still residue are completely precipitated, the still residue with precipitated by-products will be discharged and transferred to the centrifuge 4 for centrifugation. The solid obtained after centrifugation, i.e., solid waste, is transferred to the solid waste storage tank 41 for temporary storage. The centrifuged mother liquor obtained by centrifugation in the centrifuge 4 is mainly waste acid water containing organic matter, and these centrifuged mother liquors are then transferred to the still 3, combined with the subsequent waste water, and then distilled.

[0042] The present application provides an organic waste acid water treatment device, which extracts the organic in the organic waste acid water by using an extractant, separates and recovers the organic matter, and simultaneously sets a distillation kettle 3 to distill the aqueous phase after extraction, distills and recovers the acid-water mixture in the aqueous phase, cools and precipitates the kettle residue in the distillation kettle 3, and separates the solid waste and the centrifugal mother liquor by centrifugation, and recycles the centrifugal mother liquor and recycles it by using the distillation kettle 3. The device of the present application uses the above-mentioned equipment in coordination, and classifies and recycles the organic waste acid water generated in the synthesis of piperonal, which has the advantages of saving resources and reducing pollution, and overcomes the disadvantage of the existing method for treating waste acid water in the synthesis of piperonal, which fails to fully recycle the recyclable materials and causes waste of resources.

[0043] like Figure 2 As shown, optionally, the extraction kettle 2 includes an extraction kettle body 21 and a filter 22;

[0044] The filter 22 is disposed at the lower part of the extraction kettle body 21 and is connected via a connecting pipe 23;

[0045] The connecting pipe 23 is provided with a valve 100 .

[0046] In the present application, the filter 22 is provided to intercept and filter the solid impurities mixed in the extractant, so that the output extract is clean.

[0047] In the present application, the connecting tube 23 is made of a transparent material such as glass, etc., so as to facilitate observation of the flow of the lower liquid phase.

[0048] like Figure 2 As shown, optionally, a stirring paddle 211 is provided in the extraction kettle body 21;

[0049] The outer side wall of the extraction kettle body 21 is provided with a jacket.

[0050] In the present application, a stirring paddle 211 is provided in the extraction kettle body 21 to facilitate mixing of the waste acid water and the extractant in the kettle through stirring, thereby improving the extraction efficiency.

[0051] When the separation rate of the oil phase and the water phase is too low or emulsification occurs after extraction by stirring, a heat exchange medium can be introduced into the jacket to increase the temperature in the kettle to promote the separation of the two phases.

[0052] like Figure 2 As shown, optionally, a balance pipe 212 is also provided on the top of the extraction kettle body 21;

[0053] The balance pipe 212 is connected to a filter box 213 .

[0054] In the present application, due to the existence of the balance pipe 212, the pressure inside and outside the extraction kettle body 21 can be balanced, ensuring that the liquid in the extraction kettle 2 can flow down smoothly, and due to the filter box 213 connected to the balance pipe 212, the extraction agent can be prevented from volatilizing and escaping from the balance pipe 212 into the atmosphere, causing adverse effects on the environment.

[0055] like Figure 3 As shown, optionally, a plurality of filter screens 221 are arranged in the filter 22 along the liquid flow direction;

[0056] The mesh openings of the multi-layer filter screen 221 are gradually reduced along the liquid flow direction;

[0057] The connection between the filter 22 and the connecting pipe 23 is a detachable connection.

[0058] The extract enters the filter 22 through the connecting pipe 23, and the solid particles in the extract are intercepted and filtered through the multi-layer filter screen 221 in the filter 22. The filtered extract is transferred to the reactor as a reaction substrate for subsequent reactions.

[0059] The connection between the filter 22 and the connecting pipe 23 is a detachable connection, which is convenient for timely replacement of the filter 22 or retroactive maintenance thereof.

[0060] like Figure 4 As shown, optionally, one end of the filter box 213 is connected to the balance pipe 212, and the other end is closed by an end cap 2131, and the side of the filter box 213 is a hollow structure;

[0061] A porous partition 2132 is provided at one end of the filter box 213 close to the balance pipe 212 , and granular activated carbon is filled between the porous partition 2132 and the end cover 2131 .

[0062] The side of the filter box 213 is a hollow structure so that the inside and outside of the kettle can be connected through the filter box 213. The porous partition 2132 supports the loaded activated carbon particles and also plays a role of ventilation to ensure the balance of air pressure inside and outside the kettle.

[0063] like Figure 5As shown, optionally, the solid waste storage tank 41 is connected to the solid waste treatment device 42;

[0064] The solid waste treatment device 42 is an incinerator or a cracking furnace.

[0065] The solid obtained by centrifugation in the present application, that is, the solid waste is transferred to the solid waste storage tank 41 for temporary storage, and then the solid waste stored in the solid waste storage tank 41 is transferred to the incinerator for incineration for harmless treatment, or the solid waste is transferred to the cracking furnace for cracking and then resource treatment.

[0066] An organic acid wastewater treatment device, the working process of which is as follows:

[0067] When in use, the waste acid water temporarily stored in the wastewater storage tank 1 is transferred to the extraction kettle body 21 of the extraction kettle 2, and then the extractant (ethylene dichloride in this application) in the extractant storage tank 20 is added to the extraction kettle body 21 of the extraction kettle 2 to a suitable liquid level. At this time, the stirring paddle 211 in the extraction kettle 2 is turned on to stir the waste acid water and the extractant in the extraction kettle body 21. The organic compounds in the waste acid water (such as piperonal, 3,4-methylenedioxyphenylethanolic acid, piperonyl ring and other organic substances) are extracted by the extractant. After the extraction and stirring in the extraction kettle 2 are completed, the stirring is stopped, and the liquid is allowed to stand for 20 to 30 minutes to allow it to be completely separated (when the separation of the oil phase and the water phase in the extraction kettle 2 is not obvious, a heat exchange medium can be introduced into the jacket provided outside the extraction kettle body 21 to heat the liquid in the kettle to accelerate its separation efficiency). Since the specific gravity of the extractant (ethylene dichloride, specific gravity is about 1.25) is greater than the specific gravity of water (specific gravity of water is 1), the extractant forms an oil phase in the lower layer. At this time, the valve 100 on the connecting pipe 23 is opened again. The oil phase of the lower layer, i.e., the extract, is released. Due to the existence of the balance pipe 212, the pressure inside and outside the extraction kettle body 21 can be balanced, ensuring that the liquid in the extraction kettle 2 can flow down smoothly. In addition, due to the filter box 213 connected to the balance pipe 212, the extractant can be prevented from volatilizing and escaping from the balance pipe 212 into the atmosphere, causing adverse effects on the environment. The extract in the lower layer enters the filter 22 through the connecting pipe 23, and the solid particles in the extract are intercepted and filtered through the multi-layer filter screen 221 in the filter 22, and the filtered extract is transferred to the extract storage tank 8 for recovery.

[0068] The upper aqueous phase in the extraction kettle body 21, i.e., the waste acid water, is pumped into the still kettle 3 through the liquid transfer pump 71, and the still kettle 3 is heated at this time (the heating method can be steam or an electric heater is set in the still kettle 3, and steam heating is adopted in the present application, i.e., high-temperature and high-pressure steam is passed into the jacket of the still kettle 3), and in the present application, for example, the temperature of the liquid in the kettle is heated to 120-140° C. At this time, the water in the waste acid water and the azeotropic mixture of nitric acid-water will be evaporated, and the evaporated gaseous substance is condensed into liquid in the condenser on the still kettle 3 (in the present application, the evaporated gaseous substance is condensed into liquid, and cooled to 30-50° C., and extracted from the condenser of the still kettle 3), and the condensate extracted from the still kettle 3, i.e., dilute nitric acid (mass concentration is less than 5%) is transferred to the dilute nitric acid storage tank 6 to prepare the dilute nitric acid of the concentration required for the reaction (in the present application, the dilute nitric acid with a mass concentration of 10% is adopted during the reaction), and the dilute nitric acid configured in the dilute nitric acid storage tank 6 can be used for the reaction in the reactor 7.

[0069] After the distillation of the acid water in the distillation kettle 3 is completed, some kettle residue that has not been distilled out still remains in the kettle. At this time, the heating of the distillation kettle 3 is stopped, and the distillation kettle 3 is cooled by circulating water. Since the residue in the kettle is the by-product generated during the reaction (such as the substance formed by the polymerization between the substrates), these substances in the kettle residue will precipitate as solids after cooling. After the substances in the kettle residue are completely precipitated, the kettle residue with precipitated by-products is discharged and transferred to the centrifuge 4 for centrifugation. The solid obtained after centrifugation, that is, solid waste, is transferred to the solid waste storage tank 41 for temporary storage, and then the solid waste stored in the solid waste storage tank 41 is transferred to the incinerator for incineration for harmless treatment, or the solid waste is transferred to the cracking furnace for resource treatment after cracking.

[0070] The mother liquor obtained by centrifugation in the centrifuge 4 is mainly waste acid water containing organic matter, and then the mother liquor is transferred to the distillation kettle 3, combined with the subsequent waste water and then distilled.

[0071] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, ordinary technicians in the field should understand that they can still modify the technical solutions recorded in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. An organic waste acid water treatment device, characterized in that: It comprises a wastewater storage tank (1), an extraction kettle (2), a liquid transfer pump (71), a distillation kettle (3), a centrifuge (4) and a mother liquid storage tank (5) which are sequentially connected in series; The distillation kettle (3) is also connected in series with the dilute nitric acid storage tank (6) and the reaction kettle (7); The mother liquid storage tank (5) is also connected to the distillation kettle (3); The centrifuge (4) is also connected to a solid waste storage tank (41); The extraction kettle (2) is also connected to the extractant storage tank (20), and the extraction kettle (2) is also connected to the liquid transfer pump (71) and the extract storage tank (8) through valves.

2. The organic waste acid water treatment device according to claim 1, characterized in that: The extraction kettle (2) comprises an extraction kettle body (21) and a filter (22); The filter (22) is disposed at the lower part of the extraction kettle body (21) and is connected to the extraction kettle body (21) via a connecting pipe (23); The connecting pipe (23) is provided with a valve (100).

3. The organic waste acid water treatment device according to claim 2, characterized in that: A stirring paddle (211) is arranged in the extraction kettle body (21); The outer side wall of the extraction kettle body (21) is provided with a jacket.

4. The organic waste acid water treatment device according to claim 2, characterized in that: A balance pipe (212) is also provided on the top of the extraction kettle body (21); The balance pipe (212) is connected to a filter box (213).

5. The organic waste acid water treatment device according to claim 2, characterized in that: Multiple layers of filter screens (221) are arranged in the filter (22) along the liquid flow direction; The mesh openings of the multiple layers of filter screens (221) are gradually reduced along the liquid flow direction; The connection between the filter (22) and the connecting pipe (23) is a detachable connection.

6. The organic waste acid water treatment device according to claim 4, characterized in that: One end of the filter box (213) is in communication with the balance pipe (212), and the other end is closed by an end cover (2131); the side surface of the filter box (213) is a hollow structure; A porous partition (2132) is provided at one end of the filter box (213) close to the balance pipe (212), and granular activated carbon is filled between the porous partition (2132) and the end cover (2131).

7. The organic waste acid water treatment device according to any one of claims 1 to 6, characterized in that: The solid waste storage tank (41) is connected to a solid waste treatment device (42); The solid waste treatment device (42) is an incinerator or a cracking furnace.

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